DE4206050A1 - Drying wetting, washing and/or cleaning agent or component - Google Patents

Abstract

In drying wet wetting, washing and/or cleaning agents (IA) and/or components (IB) of these and their aq. solns. and/or suspensions with superheated steam (II), which is recycled after removing the fraction of water vapourised in the drying stage, (II) leaves the drying zone at a temp. of min. 150 (esp. min. 180) deg.C and the internal pressure of the (II)-filled system is at or esp. above normal to prevent air entering, e.g. at sites of damage, the internal pressure pref. being under ca. 50 mbar gauge. (I) may be zeolite cpds., esp. NaA zeolite. Pref. the starting material is spray dried through nozzle(s), e.g. with rotating discs, and the inlet temp. (Ti) of (II) is min. 250 deg.C. To produce high bulk density, Ti is min. 325, esp. min. 350 deg.C and the amt. (Wv) of water vapourised is min. 300 (esp. min.) 400 kg/m2.h w.r.t. the cross-section of the drying zone. To produce the bulk density, Ti is max. 280 deg.C and Wv is 100-250 kg/m2.h. In both cases, the (II) throughput is 1.0-4.0 (pref. 1.5-3.0, esp. 1.8-2.5) m3/m2.s. Additives (III) may be incorporated in the incompletely dry prod. to bind the residual water (partly), so that the dry prod. has storage-stable bulk and free-running property and (III) pref. are (partly) added to the aq. soln. or suspension before drying.

Description

The invention relates to a new form of washing and / or cleaning-active anionic surfactant concentrates in the form of solid trickles capable powder and / or granules. The invention has been found in particular the task of washing and / or cleaning active To make anionic surfactant compounds available in one form, so far in the combination of substance properties in this way are not available. The invention wants in particular finely particulate powders and / or granules with any adjustable Anionic surfactant content - which is practically related to the pure surfactant wise surfactant mixture should be enough - provide that are characterized by low or no dust, high and adjustable bulk densities that are well over 150 g / l can lie and at the same time an optimized solution keep in aqueous washing and / or cleaning liquors.  

In an important embodiment, the invention wants such Provide anionic surfactants and / or anionic surfactant mixtures that is characterized by virtually unlimited availability can be at a low level of the cost price, today's high-quality requirements for ecologically compatible Optimally correspond to surfactants or surfactant components and are therefore particularly suitable for making a significant contribution to Exchange of anionic surfactants based on To perform alkylbenzenesulfonates.

The tasks according to the invention go in special embodiments position, known anionic surfactants from starting materials of vegetable and / or animal origin as an essential compo nents of the new non-dusting anionic surfactant concentrates available close. However, the invention is not based on these starting materials restricted of vegetable and / or animal origin. Also ent speaking, in particular ecologically compatible compounds syn are of primary origin and / or mixture com components in the sense of the action according to the invention.

The difficulties of the task according to the invention are addressed the following problem understandable, which as exemplary The following is to be understood: The specialist knowledge of washing and / or Today, cleaning agents have a wide range of ecological acceptances tables sufficiently available in quantity and also sufficient inexpensive anionic surfactant components from the field of sulfates and / or sulfonates of oleophilic organic components such as fatty acid ren, fatty alcohols, sufficiently long-chain olefins and / or alkanes and the same. The class of Half ester of sulfuric acid with fatty alcohols, in particular longer chain saturated fatty alcohols, which under the concept of Fatty alcohol sulfates (FAS) play an important role, which differs from this dissipative fatty alcohol ether sulfates (FAES), which are produced by alkoxylation,  in particular ethoxylation and / or propoxylation of fatty alcohols and subsequent sulfation of the alcohol components thus formed can be produced.

Other important representatives of anionic surfactants common today fall into the class of sulfonated fatty acids or their wash-active salts and the associated sulfonated fatty acid esters. Known surfactants from the last-mentioned class of substances are the alpha-sulfofatty acid methyl esters or their salts (MES) and the alpha-sulfonated carboxylic acids or their wash-active salts derived therefrom by ester cleavage and / or direct alpha-sulfonation of fatty acids or their wash-active salts Salts "have become known. All of these anionic surfactant compounds listed here only by way of example contain longer-chain organic residues, for example in the range from C _8-24, in particular C _12-18, and are known mixture components in detergents and cleaning agents, in which they are usually mixed with other surfactants, in particular non-surfactant character, with organic and / or inorganic framework or builder substances and other conventional mixture components.

To date, there are considerable difficulties Anionic surfactant concentrates of this type in the form of solid, free-flowing and in particular dust-free powder and / or granules are available that have a high bulk density and that of In practice, high and rapid dissolving power in aqueous Own fleets. For the broad applicability of for example vegetable and / or animal-based anionic surfactants Sulfate and / or sulfonate based the form of supply as dust-free pourable and free-flowing fine powder or granules high resolution speed is the ideal solution. Aqueous pastes, like they in the manufacture of the anionic surfactants involved here  Bring compounds as primary reaction products often occur for technical processing multifaceted problems, both from Considerations about the stability than the handling of this form of offer. Alkyl sulfate pastes are on the one hand at risk of hydrolysis and on the other all anionic surfactant pastes show strong viscosity fluctuations in Ab dependence on the solids content of the respective aqueous paste to the impossibility of pumping the watery pastes and pipes transport and thus dose, for example.

It is not surprising in this context that numerous Proposals exist, anionic surfactants of those affected according to the invention Type to convert into solid form. In particular, here Compounds suggested that mixed with the anionic surfactants Dispersants, solubilizers and / or simply water-soluble Contain salts. It is necessary to use these auxiliary substances in connection with the production of dry forms of supply the state of the art, because the previous drying technology by hot drying in spray towers and / or in a fluidized bed Anionic surfactant products of limited utility. Schwie The following are particularly important: The poor solubility and gelling tendency of important surfactant components also contributes to convert them into a fine particulate dry state equally delayed soluble dry powders. The production such dry powder leads, for example, in the spray tower when used even moderate levels of anionic surfactant in the feed extremely dusty powders. This will cause secondary interference triggered to a considerable extent, for example at Her Position and handling of such dry powder the application of breath protective masks necessary.

However, a particular difficulty lies in the subsequent following phenomenon: anionic surfactant compounds of the type described can in the drying technology known per se in  Hot air or in hot fuel gases in the usual today Spray tower technology only for low bulk powder products weight to be worked up. Also the use of help substances, for example inorganic salts as weighting agents, leads to a limited increase in the adjustable bulk seal the dry surfactant powder. The bulk densities are often less than 100 g / l. When trying to optimize the process for example, in the case of dry powder based on TAS densities of maximum 130 g / l can be set. Di-salts of previously described type can also be mixed with auxiliary substances as dry powder not even with such bulk densities produce. Here is the bulk density achievable on an industrial scale usually well below 100 g / l.

The applicant describes DE-A 40 30 688 in her earlier application a process for the production of finely divided solid bulk or wise pourable recyclable materials or mixtures of materials for network, Detergents and / or cleaning agents from their aqueous preparations, where superheated steam is used as a drying hot gas stream sets and the drying of the particulate material before its Ge risk is terminated by thermal action. Required If necessary, the storage-stable bulk or Free flowing of the partially dried material in this way by Zu Ensure set of such mixture components that are used for binding limited amounts of water are capable.

In the applicant's older German patent applications P 42 04 035.3 and P 42 04 090.6 are simplified and improved Process for drying valuable materials for washing and / or cleaning described with superheated steam. The teaching of The present invention described below ties in with the Disclosures of these earlier applications for property rights by the Applicant. For the purpose of the disclosure of the invention, the  Teach these three older applications expressly to the counter made the present disclosure of the invention.

Subject of the invention

The present invention relates to the following ge described anionic surfactant concentrates in the form of solid, free-flowing Powders and / or granules, which are also mixed as a compound further ge for use in detergents and / or cleaning agents suitable auxiliary and / or recyclable materials can be present and through Drying of corresponding water-containing preparations under Aus Formation of the powder and / or granule form have been produced.

In the sense of the teaching according to the invention, these are anionic surfactants concentrates are now characterized in that they contain the anionic surfactant connections at least partially in the form of their washing and / or contain cleaning-active salts, with bulk densities of little at least about 150 g / l and by hot drying the water containing preparations with superheated steam as the drying gas have been produced. Preferred bulk densities of this anion surfactant concentrates are at or above about 200 g / l, preferably as at or above about 300 g / l and especially at least about 350 g / l.

The anionic surfactant concentrates according to the invention continue to excel in particular from the fact that they are at least low in dust, in the be preferred embodiment are practically completely dust-free. You can characterized in a preferred embodiment be that to adjust these material properties - also one finest particles - as a mixture constituent dust-binding Contain auxiliaries and / or recyclables. In addition to or instead of this According to the invention, the measure can also be dust-free  Regulation of the residual water content in pourable and pourable goods be provided.

In a further embodiment, the invention relates to the Ver drive to the production of anionic surfactant concentrates with the aspired to combination of fabric properties as outlined above. Finally, the invention relates to a further embodiment the use of these anionic surfactant concentrates in dry form in ins special aqueous washing and / or cleaning agents, in particular for at least partial exchange for anionic surfactants on ABS Base.

Details of the invention

Surprisingly, it has been shown that compliance with the Element combination defined according to the invention and, if appropriate taking into account those detailed below Additional elements becomes possible, solid anionic surfactants and corresponding ones Anionic surfactant concentrates with the target sum of product properties equip or manufacture, which for years tenths are desired by experts, so far in this combination tion but could not be realized. The anionic surfactants Materials can be produced in the finest powder form by spray drying be put. The resulting powders are also dust-free like the one practically the only way out according to old technology see surfactant granules, their production from previously obtained Powder according to old technology be an additional step forced. Draw the anionic surfactant powders defined according to the invention are characterized by high bulk densities, which make handling, the packaging and transport of this form of offer makes sense and make it economically viable. At the same time, they are adjustable high bulk densities in the sense of the production of dry forms of supply for detergents and cleaning agents as  so-called heavy powder important for immediately usable Mi components. After all experiences of the old technology then such a form of supplying the anionic surfactant solids but with the disadvantage of being difficult or at least delayed Dissolvability in aqueous liquors. According to the invention this disadvantage no longer exists or is at least in one mitigated to the extent that restrictions on the practical Handling and utilization of those defined according to the invention Anionic surfactant concentrates are no longer available.

In a preferred embodiment, the content of it anionic surfactant concentrates according to the invention in washing or detergent-active surfactants at least about 20 wt .-% and above preferably at least about 30% by weight, based in each case on fine-grained solid material. Basically, the surfactant solids as such form the powder or granulate. Here in practice, however, it must be taken into account that from Her position of the anionic surfactants on an industrial scale as a rule limited amounts of residual components - inorganic salts, not sulfated residues and the like - as acceptable in practice or irrelevant contamination in the surfactant solid lie. Accordingly, surfactant granules are special preferred, the active content of anionic surfactants in the range of sth is 35 to 95% by weight. Within this range again such substances or mixtures of substances may be preferred in which the surfactant components make up more than 50% by weight -% by weight as for related to fine-grained solid material.

The anionic surfactant components present in these solids can certain individual recyclables of the type mentioned can be, but also practically any mixes of value substances of the surfactant class mentioned here are available. The term The "surfactant mixture" can be understood in several ways:  Already within a selected class - for example the Fatty alcohol sulfates and / or fatty acid sulfonates are usually located no individualized substance in the sense of a selected connection in front. Processing of feedstocks vegetable and / or tie origins, but also the processing of corresponding synthetics tical source chemicals leads to valuable substances of the type concerned a certain range in the composition - for example regarding the C number in the fatty alcohol and / or fatty acid residues.

However, the term “surfactant mixtures” in particular also includes, in the sense of the definition according to the invention, the targeted combination of anionic surfactants with fundamentally different structures. For example, it may be expedient to blend the classic wash-active anionic surfactants based on TAS with anionic surfactant dispersants, which may be based, for example, on comparatively shorter chain sulfates and / or sulfonates. Other examples of at least two different types of anionic surfactants are mixtures of di-salts on the one hand - ie alpha-sulfofatty acid salts, for example the chain length of C _14-20 , and other anionic surfactants based on TAS and / or based on alkyl ester sulfonates, especially methyl ester sulfonates ( MES).

To solve the subtask dust-free powders and / or granules To provide, the invention provides two solutions that can also be used in combination.

One approach is based on the proposal, targeted use of the residual water content of the goods to be dried. Depending on the nature of the solid material present in the individual case can be dust-free by regulating the residual water in the dry material become at least largely accessible.

The teaching of the invention provides an important embodiment however, that the anionic surfactant concentrates additional components in  may contain varying amounts, primarily in the invention In order to eliminate dust formation or as dust binding aids are to be viewed. The invention includes here however expressly the incorporation of such auxiliary substances, which ih on the other hand, valuable materials in the sense of use in washing and / or cleaning means or the joint use with the represent the respective anionic surfactant components concerned.

In this embodiment, the finely particulate are characterized pourable and free-flowing anionic surfactant concentrates of the invention by that they as dust-binding auxiliaries and / or valuable materials Mi contain components in preferably homogeneous mixture, the at room temperature - possibly in the presence of limited residue Amounts of water - liquid and / or at least sticky own and preferably in such amounts in the surfactant Are incorporated concentrate that the required dust-free ge is guaranteed without the bulk and pourability sustainable hinder.

Suitable dust-binding auxiliaries can be used especially in rooms temperature water-soluble, water-emulsifiable and / or water be swellable mixture components, which in turn are monomer compounds dung, oligomer compounds and / or suitably selected polymer connections are. Before going on characteristic examples of such Auxiliary or recyclable materials used as mixture components is going to be based on the teaching according to the invention here The working concept explained: The auxiliary substances can be their water solubility or water emulsifiability, in any case but also because of their water swellability to be homogeneously absorbed into it Work in the drying mixture of active ingredients based on anionic surfactants. Becomes in the subsequent drying stage in the sense of hot steam drying from the aforementioned and to complete the Erfin disclosure disclosures cited earlier applications by the applicant  water-containing feed material then in the superheated steam flow par ticularly and in particular finely divided and under the one effect of the superheated steam is so reliable and even mixing of these dust-binding aids in everyone Particles ensured in an even distribution. Through the liquid, viscous or at least sticky consistency of the Excipient occurs in the finally dried particle dust-binding effect of this additive in the foreground. By a suitable choice of quantity in the active substance mixture used can be different on the other hand, it must be ensured that the desired state the stick-free pourability or flowability is also maintained for any length of storage period. The mixing ratios to be set in each individual case are by simple experiments taking into account the be the specialist knowledge found.

In the following, representative representatives for such dust-binding auxiliary or recyclable materials for abmi listed with the anionic surfactant components:

Suitable water-soluble and flowable under normal conditions Components are polyfunctional volatile alcohols approximately their oligomers, although here for reasons of cost Special glycerin or corresponding oligoglycerols Meaning can be. Further examples of corresponding flows capable and / or at least under the influence of residual water Appropriate stickiness-imparting compounds are mixture components ten such as oligomers and / or polymers of ethylene glycol and / or Pro pylene glycol. In particular polyethylene glycols - for example one Molecular weight range up to about 10,000, preferably up to about 7,000, can be valuable materials in the sense of the inventive action that - as well as the previously mentioned representatives glycerin and / or Oligoglycerins - not only cause the desired dust binding,  but also solubilizer and / or valuable substance in Frame of detergents and cleaning agents are. Typical representatives for but suitable auxiliaries are also mono- and / or oligoglycosides, being exemplified, glucose, oligo glucose, sugar such as succrose or correspondingly higher ring numbers comprehensive sugar, or sugar compounds, up to corresponding polymer compounds on the type of starch and / or partially degraded starch and starch derivatives. All connections this type is known to ge particularly in the presence Ringer amounts of water through a more or less pronounced Stickiness, in practical use of washing and cleaning these com components immediately absorbed by the aqueous washing liquors and disrupt the desired washing or cleaning processes Not.

In this context, reference should be made to a further possibility of the design of the anionic surfactant compounds discussed here: Today, selected glycoside derivatives are becoming increasingly important as wash-active compounds, which are particularly noteworthy as natural substance-based substances of this type. The classes of the alkyl polyglycoside compounds (APG) and the esters or partial esters of glycosides, sugars and the like with preferably longer-chain fatty acids are addressed. Glycoside compounds of the type concerned here have a pronounced non-surfactant character. They are also characterized by pronounced performance-enhancing synergisms when mixed with anionic surfactants. As solids, glycoside compounds of the type affected here are generally sufficiently hygroscopic as solids, despite their substitution with hydrocarbon residues of, for example, C _8-20 , in particular C _10-18 , that they can be mixed with the anionic surfactants and when they are mixed Drying appropriate aqueous slurries can also take over the function of reliable binding of powdery components. The resulting diversity in increasing the value of a corresponding anionic surfactant / nonionic surfactant mixture requires no further explanation.

Suitable mixture components for the reliable removal of the Dust problems are also oligomeric and / or polymeric mixtures components, which in turn are preferably at least water-swellable and / or are also water-soluble. Here too comes a multitude of Representatives into consideration, who in the context of usual washing and cleaning important importance. As examples named: polyvinylpyrrolidone (PVP), polyvinyl alcohol (PVA), poly carboxylate compounds, in particular of synthetic origin, the for example by polymerization or copolymerization of (meth) acrylic acid and maleic acid or maleic acid anhydride can be obtained and as a so-called builder compo play a significant role in today's laundry detergents play. Another important example of the connection class of the latter type are oligo- containing carboxyl groups or polyglycoses as they are caused by the targeted oxidation of Starch with the introduction of the carboxyl group in 6-position on the gluco sering are available. Corresponding ones are still suitable water-soluble and / or water-swellable cellulose derivatives, such as Methyl cellulose, carboxymethyl cellulose, hydroxyalkyl celluloses, such as Hydroxyethyl cellulose and the like.

These representatives can only be listed as examples by any other mixture components with the specified Material properties - especially sufficient water solubility or water swellability, as well as sufficient non-cans activity under the reprocessing conditions in the superheated water steam flow - supplemented and / or replaced. This also applies here relevant general expertise.  

A certain additional class of auxiliary substances is in this Relationship received separately: As mixture components can in particular, be flowable even under normal temperature conditions or sufficiently sticky non-surfactant components in Come into consideration, the nonionic surfactants already described above The base of the glycoside ethers or esters cannot be assigned are. The fatty alcohol class is only an example ethoxylates with, for example, 2 to 40 EO units, in particular 2 up to 20 EO units in the molecule or on corresponding ones Ethoxylates of fatty acids, fatty amines, carboxamides and / or Alkanesulfonamiden referenced. The special teaching of the beginning named DE-40 30 688 of the applicant names in connection with the drying processes disclosed there under the influence of over heated water vapor numerous important subclasses and special Types as examples of such non-surfactant components. The Teaching of the present invention is inter alia about the open tion of the older application insofar as it is according to the invention is now focused on suitable nonionic surfactant components with sufficient fluidity or stickiness in Ge presence of residual water for the safe binding of unwanted Use of dust in the finished product, but at the same time So far only in the powder dry state as extremely dusty Active ingredient preparations accessible anionic surfactants in high solids to be able to provide substance concentrations.

Washing and / or clean are suitable as anionic surfactant compounds Much active representatives of this class of substances, as they do are available to experts today. Natural product based mate As already stated, materials are just as suitable as corresponding ones Secondary products of synthetic chemistry. Preferred anionic surfactants are characterized by increased ecological compatibility and are in particular for the partial and / or complete exchange of the anionic active ingredient based on ABS.  

Particularly important anionic surfactant compounds for teaching the invention are fatty alcohol sulfates, fatty alcohol ether sulfates, olefin and / or alkane sulfonates, fatty acid ester sulfonates, sulfated fatty acid triglycerides and / or glycerin fatty acid partial ester sulfates. Another important example of anionic surfactants in the sense of the action according to the invention are succinic acid half-ester sulfonates which have a sufficiently oleophilic residue in their ester grouping - for example a fatty alcohol residue with 6 to 20 C atoms, in particular 10 to 16 C atoms. Particularly important representatives of the fatty acid ester sulfonates are the known anionic surfactants based on alpha-sulfofatty acid lower alkyl esters or their salts, the most important representatives of which are the alpha-sulfofatty acid methyl esters (MES). Characteristic representatives for fatty acid sulfonates are alpha-sulfofatty acids or their washing or cleaning salts, which are known in the art as "di-salts" and are accessible from free fatty acids and / or from corresponding alpha-sulfofatty acid esters by ester cleavage. Sulfated fatty acid triglycerides are known to be reaction products of natural fats and / or oils with in particular SO ₃ , which are obtained as multicomponent mixtures of active ingredients from sulfates and sulfonates and are described, for example, in the applications for property rights by the applicant DE 39 36 001 and 39 41 365.

The washing and / or cleaning active anionic surfactants are more common as in the form of their alkali and / or ammonium salts respectively as soluble salts of organic bases. Particularly important Alka lis salts are known to be the sodium salts and the corresponding ones Potassium salts.

The teaching of the invention includes the blending of the anionic surfactants bindings and their blends with the previously listed Mi research components, in particular of an organic nature, also in Ab  mixture with inorganic components. Here it can preferred corresponding components from the field more common Components of detergents and / or cleaning agents act that expediently also homogeneously in the powder and / or granules are incorporated. As examples of such water-soluble anor ganic mixture components are water-soluble salts such as Na trium carbonate, sodium bicarbonate and / or sodium sulfate but also water-soluble sodium silicates, especially those for washing and Cleaning agent named typical water glasses. In addition to or instead of such water-soluble inorganic components can water insoluble mixture components in the powdered anionic surfactant agglomerates must be incorporated. An example is: Synthetic zeolite compounds, in particular zeolite NaA in washing medium quality and a calcium binding capacity in the range of 100 to 200 mg CaO / g - compare the information in DE 24 12 837. Die Special feature for anionic surfactant concentrations designed according to the invention The use of such insoluble anorga becomes a problem nical components: For example, TAS combined with zeolite NaA a conventional spray drying process the wash-active TAS component tightens and in such a thin layer on the zeolite particles that in the following substantial use of washing power no longer applies can train in the aqueous fleet. In the de finished and produced in the context of the teaching of the invention This negative effect of the addition of zeolite is anionic surfactant concentrates not ge or at least to a very greatly reduced extent give. Further examples of possible water-insoluble mixed compos elements are fine-particle swellable layered silicates of the type corresponding montmorilonite, for example bentonite.

The possible embodiments of the superheated steam drying process rens will refer to the older registrations mentioned and in particular the applications according to German patent applications P 42 04 035.3 and  P 42 04 090.6. To complete the open-ended invention Agreement in the context of the present application is only here dealt with a selection of particularly important process parameters gene:

Enable the working conditions of the method according to the invention the use of high temperatures of the circulated water vapor phase in the area of the drying step of spray drying. In As a rule, the working temperatures of the steam used are higher half 150 ° C and preferably at least about 200 ° C in the gas phase. Working temperatures of 250 ° C and above can be be particularly interesting, in particular the temperature range of at least 300 ° C, in particular 300-380 ° C into consideration is coming. For many cases, working temperatures are in the range of around 270-350 ° C particularly suitable in the water vapor phase. Thereby be all of these temperature specifications each relate to the temperature of the spray zone supplied in cocurrent or countercurrent on Opti times temperature of heated steam flow. In a known way Way decreases in the course of lingering with the wet relationship wise damp the temperature of the water vapor. Largely en ergetische considerations - in particular also to the intended Further use of the partial steam flow to be removed - determine the proportions between the liquid to be evaporated amount and the supplied amount of superheated steam. Embodiments are possible here which only have a limited extent Lowering the steam temperature after leaving the spray zone, for example to include values in the range of around 190-250 ° C, while in other embodiments, a further utilization of the thermal energy of water vapor up to a decrease in Steam temperature close to the condensation temperature under Ver driving conditions -100 to 110 ° C - appropriate or before can be partaking. These detailed questions are answered in detail by the Design of the circular process in its entirety  co-determined. Corresponding considerations apply to the use of superheated steam as hot gas in an optionally pre- post-drying stage in the fluidized bed process. That too the given numerical values apply accordingly.

Basically applies to these considerations that in the closed Sy stem is operated with a steam cycle, the evaporated water portion of the feed is withdrawn during the the amount of energy given off especially in the drying step Circulation current in a direct or preferably indirect way again is fed. The subtracted water vapor is after the Cleaning of carried good parts in an important execution tion form used as process steam for other use, after if desired, the pressure and temperature of this steam Partial stream have been adjusted to the conditions required there are. In another embodiment of the Ver driving it may be appropriate to take at least a portion of this condensed steam partial flow to condense, for example a wet washing of the withdrawn partial steam stream and its cleaning effect of carried shares. The resulting one aqueous liquid phase together with those present therein circled recycled materials in the drying process leads. In this context it is possible, for example, vaporous portions of the circled gas stream for To concentrate such a washing liquid phase. The returned liquid parts with recyclable content can fed directly to the spray zone or first with the aqueous Fresh preparations mixed and in this form for drying in the spray zone can be entered.

A particularly interesting embodiment of the invention Teaching sees the recovery and utilization of the heat of condensation of the water vapor removed from the circuit. By  The use of suitable work steps can be the recycling also the low proportions of recyclable materials can be ensured the discharged superheated steam flow the primary circuit of the Have left steam. Here, for example, can be exploited the heat of condensation of the discharged steam as follows to be worked:

In a preferably multi-stage evaporation plant is used the heat of condensation of the subtracted steam the steam concentrated condensate. The remaining concentrate is returned to the primary process circuit. In particular can this residual concentrate is to be dried by superheated superheated steam Recycled slurry are added.

If necessary, condensation from the primary cycle of discharged superheated steam if necessary falling residual gas phase loaded with the smallest amounts of recyclable material subsequent processing step - for example a scorch treatment, treatment in biofilters or in washing systems will. By such a combination of measures of a practical complete recycling of the respective partial flows and the he enables the reliable destruction of last traces Procedures according to the invention in the field concerned here industrial production for the first time the possibility of recyclables and Mixtures of valuable materials from the field of washing and cleaning agents Waste gas-free and free of loaded wastewater.

Even under the working conditions according to the invention, the dry on the one hand as spray drying and / or on the other hand also as drying in a fluidized bed be taken. Comparatively high-water operational material Lien are, for example, as flowable and sprayable aqueous Solutions, emulsions and / or suspensions of those to be dried  Recyclables or mixtures of recyclables. Feed materials this type will be in an important embodiment of the known technology of spray drying. The spray Drying can take place in appropriately equipped spray towers be carried out in current or countercurrent mode. The application the countercurrent principle is also within the scope of the invention Working with superheated steam as the hot drying gas in the Usually preferred.

When working under the conditions of spray drying it will according to the invention preferably the direct or preferably indirect Energy input for supplying the vaporization energy into the steam cycle at least predominantly outside the drying zone increase. In this way it becomes conventional spray Drying known result ensures the flowable wet Feed material in fine particle form without significant sticking the particles with each other or at least under a controllable Dry up the particle size setting. The outside of the Spray drying zone on the steam circuit energy input can be in any known form of indirect heat be carried out. The use of Pipe bundle systems mentioned, on the one hand any of heating gases Origin and on the other hand - but separate from these heating gases - are flowed through by the steam flow to be heated.

In a particularly important embodiment of the invention this indirect energy input into the steam cycle stream by means of one or more integrated burners with indirect heat transfer Carried out on the steam flow, the burner side hot combustion gases directly into the heat exchanger be conducted, which is integrated into the steam cycle stream. The The temperature of the combustion gases can range, for example from about 400 to 1,000 ° C and especially in the temperature range of  about 650 to 960 ° C. For optimal heat utilization and therefore to reduce the cost of the overall process, it may be appropriate to Proportionate, preferably as far as possible, recycling To provide flue gases. For example, at least 30% by volume and preferably more than 40 vol .-% of the hot flue gases after the Leaving the integrated heat exchanger in the circuit to further energy recovery can be recycled. Preferably the amount of flue gas circulation is more than 60 vol% and often in the range of about 70 vol .-% of Ver supplied combustion gases. All the usual Brennga are used to operate the burner se, in particular natural gas or comparable lower hydrocarbons substances or hydrocarbon mixtures and / or water suitable for fabric.

On the other hand, the drying principle according to the invention is within the scope a fluidized bed drying is used, so here the required heating of the drying gas based on steam both outside the drying zone as well as with heat exchanger elements be integrated into the fluidized bed. You can do that too these two mechanisms of gas heating are linked will.

The preferred working according to the invention in the area of normal pressure enables the comparatively uncomplicated operation also in industrial plants with the required high material throughputs per unit of time. The measure preferred according to the invention of the light raised internal pressure reliably prevents the unwanted Break-in of foreign gas, especially air, into the water steam-filled circulatory system. Secondary damage to the aspired high quality product quality can be reliable be excluded. Suitable working prints are, for example in the range up to about 150 cm water column, expediently up to about 75 cm Water column and preferably below 50 cm water column. The  Range of about 5 to 15 cm water column system internal pressure can be be particularly preferred. Drying with superheated steam in the The principle of the teaching according to the invention is of course also in principle Negative pressure possible, especially in the area of moderate negative pressure, but then requires an increased technical effort for security the exclusion of possible damage in the circulatory system, which would trigger unwanted air ingress.

Examples example 1

In a pilot spray tower on a pilot scale of the "Minor Production" type from Niro-Atomizer, a slurry of the sodium salt of a C ₁₆ / C ₁₈ -alpha-sulfofatty acid with a dry matter content of 36.5% was converted into a surfactant powder with a bulk density of 370 g / l converted. The following key figures were measured on the starting slurry:

Epton wash active substance 26.3%, based on slurry.

Unsulfonated fatty acid 2.09%.

Sodium sulfate 3.1%.

Sodium chloride 2.2%.

Degree of sulfation 89.6%.

The following operating parameters have been set:

Speed of the rotary atomizer 25,000 revolutions per minute.

Steam inlet temperature around 300 ° C.

Steam outlet temperature around 200 ° C.

Tower vacuum 16 mbar.

Feed pump pressure 0.2 bar.

Feed temperature 80 ° C.

Feed quantity 8 kg per hour, increased during spraying to 18 kg per hour.

Steam amount about 500 m ³ per hour.

The product obtained had a dry matter content of 99.8% and a bulk density of 370 g / l. It showed very cheap resolutions properties when added to water.  

Example 2

The procedure was as in Example 1. It was dried in a slurry with a solids content of 36%, which contained the above-mentioned sodium salt of a C ₆ / C ₁₈ -alpha-sulfofatty acid (with admixtures) and polyethylene glycol with a molecular weight of 2000 in the weight ratio of the dry substances of 9: 1. The tower inlet temperature was 300 ° C; the outlet temperature at 210 ° C; all other parameters were comparable. The product had a dry matter content of 99% by weight; the bulk weight was 290 g / l.

Claims (13)

1. Anionic surfactant concentrates in the form of solid, free-flowing powders and / or granules, which can also be present as compounds in a mixture with other auxiliaries and / or valuable materials suitable for use in detergents and / or cleaning agents, and by drying appropriate aqueous preparations with formation of the powders - And / or granules have been produced, characterized in that they contain the anionic surfactant compounds at least partly in the form of their washing and / or cleaning salts, have bulk densities of at least about 150 g / l and by hot drying the water-containing preparations with superheated steam have been produced as drying gas. 2. anionic surfactant concentrates according to claim 1, characterized in that they have bulk densities above about 200 g / l, preferably above half about 300 g / l and in particular at least about 350 g / l exhibit. 3. anionic surfactant concentrates according to claims 1 and 2, characterized shows that by using dust-binding auxiliary and / or recyclables and / or by regulating the residual water content as essentially dust-free pouring and pouring capable goods are trained. 4. anionic surfactant concentrates according to claims 1 to 3, characterized records that their content of washing and / or cleaning active Surfactants at least about 20 wt .-%, preferably at least about 30% by weight and in particular in the range from about 35 to 95 % By weight, and in a particularly preferred embodiment form the content of surfactant components more than 50 wt .-% - % By weight based on fine-grained solid matter.   5. anionic surfactant concentrates according to claims 1 to 4, characterized records that they as dust-binding auxiliaries and / or recyclables Mix components preferably in a homogeneous mixture ten as such at room temperature - optionally in Ge presently limited amounts of residual water - liquid and / or we have at least sticky properties and preferably in such amounts are incorporated into the surfactant concentrate that the required freedom from dust is guaranteed without the bulk and hinder free-flowing ability in the long term. 6. anionic surfactant concentrates according to claims 1 to 5, characterized records that as dust-binding auxiliaries at room temperature water-soluble, water-emulsifiable and / or water-swellable mo nomere, oligomeric and / or polymeric mixture components such as Glycerin, oligoglycerins, polyethylene glycols and / or poly propylene glycols, mono- and / or oligoglycosides respectively corresponding glycoside compounds, in particular washing and / or cleaning-active alkyl glycoside compounds, water swellable and / or water-soluble oligomer and / or polymer compounds such as polyvinyl pyrrolidone (PVP), polyvinyl alcohol (PVA), polycarboxylates or cellulose derivatives such as Methyl cellulose, carboxymethyl cellulose, hydroxyalkyl cellulose, but also others at room temperature and / or in the presence of Residual water flowable or sticky components with Surfactant character, in particular corresponding nonionic surfactants gene. 7. anionic surfactant concentrates according to claims 1 to 6, characterized records that it as a washing and / or cleaning active anion surfactant compounds fatty alcohol sulfates (FAS), fatty alcohol Ether sulfates (FAES), olefin and / or alkane sulfonates, fat acid ester sulfonates, especially low alpha sulfo fatty acid alkyl esters or their salts, fatty acid sulfonates,  in particular alpha-sulfo fatty acids or their salts (Di-salts), succinic acid half-ester sulfonates, sulfated fat acid triglycerides and / or glycerin / fatty acid partial ester Contain sulfates. 8. anionic surfactant concentrates according to claims 1 to 7, characterized records that the washing and / or cleaning active anionic surfactants in the form of their alkali and / or ammonium salts or as soluble salts of organic bases are present. 9. anionic surfactant concentrates according to claims 1 to 8, characterized records that at least two different anionic surfactant Types, for example FAS and di-salts or MES and di-salts, in preferably homogeneous mixing with one another. 10. anionic surfactant concentrates according to claims 1 to 9, characterized records that they are in addition to the surfactants and optionally organic mix components inorganic mix Ingredients, preferably from the range of common ingredients of detergents and / or cleaning agents - further preferred also incorporated homogeneously into the powder and / or granules tet - included. 11. anionic surfactant concentrates according to claims 1 to 10, characterized ge indicates that they are water-soluble inorganic components such as sodium carbonate, sodium sulfate and / or water glass in Abmi with the surfactant components. 12. Process for the preparation of the anionic surfactant concentrates in powder and / or granulate form according to claims 1 to 11, characterized records that aqueous solutions, emulsions and / or suspensions Sions of the surfactants or surfactant mixtures and the counter possibly also used auxiliary and / or recyclable materials  Conditions of drying with superheated steam in one Spray zone and / or in fluidized bed. 13. Use of the anionic surfactant mixtures according to Claims 1 to 11 in Detergents and cleaning agents, in particular for at least par exchange for anionic surfactants based on alkylbenzene sulfonate.